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EP0657391B1 - Bleifreie Gläser mit Kristalleigenschaften - Google Patents

Bleifreie Gläser mit Kristalleigenschaften Download PDF

Info

Publication number
EP0657391B1
EP0657391B1 EP94118661A EP94118661A EP0657391B1 EP 0657391 B1 EP0657391 B1 EP 0657391B1 EP 94118661 A EP94118661 A EP 94118661A EP 94118661 A EP94118661 A EP 94118661A EP 0657391 B1 EP0657391 B1 EP 0657391B1
Authority
EP
European Patent Office
Prior art keywords
sro
bao
zno
zro
sio
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP94118661A
Other languages
English (en)
French (fr)
Other versions
EP0657391A1 (de
Inventor
Marie Jacqueline Monique Comte
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Corning Inc
Original Assignee
Corning Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Corning Inc filed Critical Corning Inc
Publication of EP0657391A1 publication Critical patent/EP0657391A1/de
Application granted granted Critical
Publication of EP0657391B1 publication Critical patent/EP0657391B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
    • C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/078—Glass compositions containing silica with 40% to 90% silica, by weight containing an oxide of a divalent metal, e.g. an oxide of zinc
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C4/00—Compositions for glass with special properties
    • C03C4/0028—Compositions for glass with special properties for crystal glass, e.g. lead-free crystal glass

Definitions

  • This invention relates to glasses essentially free from lead displaying the physical characteristics of lead-containing crystal glasses.
  • crystal occupies an exceptional place: its brightness, its density, and its sonority make it a much esteemed material. In addition, it exhibits the characteristics of formability at moderate temperatures, of having a long working range, and of being able to be easily cut and polished.
  • lead oxide in the glass composition.
  • lead is a toxic, and nowadays is considered problematical for handling, manufacturing and use, especially the latter, as lead in the glass can migrate into food in contact with the glass, and lead poisoning, particularly after contact with an acid medium, for example, fruit juices or alcohol.
  • the present invention solves the problem by lead free glasses suitable for use as tableware and/or decorative crystal glassware meeting the following requirements:
  • the invention relates to glasses essentially free from lead (no lead additions to the batch, except as incidental batch impurities) having the following compositions, expressed in terms of weight percent on the oxide basis.
  • the present invention provides glasses essentially free from lead characterised in that they exhibit a density of at least 2.9 g/cm 3 and an index of refraction of at least 1.545, and which consist essentially of the composition as defined above, but subject to the proviso that the specific glasses of the compositions disclosed in Examples 6, 16, 18 and 19 of United States Patent No 4,277,286 (which are set out below) are excluded.
  • the present invention provides tableware and/or decorative crystal glassware consisting of glasses essentially free from lead characterized in that they exhibit a density of at least 2.9 g/cm 3 and an index of refraction of at least 1.545, and which consist essentially of the composition as defined above, but not subject to the proviso based on Examples 6, 16, 18 and 19 of United States Patent No 4,277,286.
  • BaO, ZnO and SiO 2 are utilized in order to obtain the required density and index of refraction.
  • BaO is the most effective component for raising the index and the density. In addition, it provides a lower cost increase than ZnO and SrO. However, its level must be maintained below 21% to avoid unacceptable devitrification.
  • ZnO is preferred to SrO because SrO tends to give a yellow color to the glass, its cost is relatively high, and it raises the thermal expansion of the glass more than ZnO.
  • the level of SiO 2 +Al 2 O 3 +ZrO 2 must be maintained at least 55% to impart acceptable chemical durability to the glass.
  • LiO 2 plays a favorable role regarding the viscosity of the glass. However, its content is limited to 3% because of its cost.
  • the other components such as ZrO 2 , B 2 O 3 , TiO 2 , CaO, MgO, and La 2 O 3 can be added to adjust the properties of the glass.
  • ZrO 2 , B 2 O 3 , TiO 2 , CaO, MgO, and La 2 O 3 can be added to adjust the properties of the glass.
  • ZrO 2 exhibits an interesting effect with respect to the density and the refractive index of the glass. But in amounts higher than 6%, it leads to glasses difficult to melt and displaying an acceptable devitrification.
  • TiO 2 demonstrates an interesting effect on the refractive index of the glass, but it leads to a yellow coloration in the glass, this color being more intense as the level of Fe 2 O 3 comprising an impurity in the batch materials increases. Its amount must be limited to 3% and is preferably essentially excluded when a colorless glass is desired.
  • a level of Fe 2 O 3 less than 150 ppm is, for example, desirable.
  • Coloring components such as the transition metal oxides or the rare earth metal oxides can also be added in a total amount less than 0.1% to mask the tint imparted by the impurities. These components can also be added in higher amounts to color the material, if one desires a colored glass.
  • As 2 O 3 and Sb 2 O 3 can also be added in the usual proportions to perform their customary role as fining agents.
  • the preferred glasses of the invention have the following compositions, expressed in terms of weight percent on the oxide basis: SiO 2 53-62 ZnO 8-13 Li 2 O 0-2 SrO+BaO+ZnO 27-32 Na 2 O 2-7 CaO 0-5 K 2 O 3-11 Al 2 O 3 0-3 Li 2 O+Na 2 O+K 2 O 8-14 ZrO 2 0-4 SrO 0-3 SiO 2 +Al 2 O 3 +ZrO 2 56-65 BaO 15-19
  • Glasses having compositions within those ranges exhibit an interesting compromise between the different properties, those related to the ease of manufacturing as well as those related to the final product.
  • the low levels of Li 2 O and SrO enable the cost of the composition to be limited.
  • the simultaneous presence of Na 2 O and K 2 O facilitates melting of the glass.
  • Lead-free glasses have also been utilized in the fabrication of faceplates for television receiver tubes in order to avoid the development of a brownish discoloration resulting from the impingement of high velocity electrons, with accompanying X-radiation, upon PbO-containing glasses.
  • the following United States patents are illustrative of such glasses: 3,464,932 (Connelly et al ), 3,805,107 (Boyd), 4,089,693 (LaGrouw et al ), 4,277,286 (Boyd et al ), 4,734,388 (Cameron et al ), 4,830,990 (Connelly), and 5,108,960 (Boek et al ).
  • the glasses disclosed therein vary in composition and properties from those of the present invention.
  • the glasses are essentially free from PbO and other readily-reducible metal oxides and consist essentially, in weight percent on the oxide basis, as calculated from the batch of: SiO 2 43-55 CaO 0-5 Al 2 O 3 0-4 SrO 2-14 ZnO 5-12 BaO 10-20 Li 2 O 0.5-3 CrO+SrO+BaO 16-30 Na 2 O 4-8 CeO 2 0.3-1 K 2 O 3-8 ZrO 2 2-8 Li 2 O+Na 2 O+K 2 O 10-18
  • CA-A-2 097 872 corresponding to US-A-5,270,269 is also directed to the production of lead-free fine crystal glassware.
  • the glasses disclosed therein consist essentially, in weight percent, of SiO 2 54-64 BaO 8-13 Li 2 O 0-3 SrO 8-13 Na 2 O 0-6.5 ZnO 5.5-9 K 2 O 0-7 BaO+SrO+SnO 22-33 Li 2 O+Na 2 O+K 2 O 8-15 wherein at least two of Li 2 O, Na 2 O, and K 2 O are present and are present in essentially equimolar ratios.
  • the BaO content of the subject inventive glasses is greater than the maximum permitted in the glasses described in the patent, and the level of SrO is lower than the minimum demanded in the glasses of the patent.
  • the present inventive glasses have no requirement that at least two alkali metal oxides be present in equimolar amounts.
  • the appended table presents examples of compositions and properties.
  • the compositions are recorded in terms of parts by weight, but, because the sum of the components totals or closely approximates 100, for all practical purposes, the individual values can be deemed to reflect weight percent.
  • 3000 grams of batch materials were melted for 4 hours at 1500°C in a platinum crucible. Thereafter, the molten glasses were formed into bars and measurements performed thereon. Whereas these examples reflect only laboratory experiments, the glasses of the invention can be manufactured in industrial plants utilizing classical glass melting and forming techniques.
  • Example 1 is the most preferred glass.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Glass Compositions (AREA)

Claims (6)

  1. Gläser weitgehend frei von Blei,
    dadurch gekennzeichnet, daß
    sie eine Dichte von mindestens 2,9 g/cm3 und einen Brechungsindex von mindestens 1,545 aufweisen und weitgehend aus den folgenden Zusammensetzungen bestehen, ausgedrückt in Gewichtsprozent auf Oxidbasis, SiO2 51-63 Al2O3 0-5 Li2O 0-3 ZrO2 0-6 Na2O 0-8 SiO2+Al2O3+ZrO2 55-66 K2O 0-12 TiO2 0-3 Li2O+Na2O+K2O 7-15 CaO 0-5 SrO 0-<8 MgO 0-3 BaO >13-21 B2O3 0-3 ZnO 5-15 La2O3 0-8 SrO+BaO+ZnO 27-34
    mit der Maßgabe, daß die folgenden speziellen Glaszusammensetzungen ausgenommen sind: SiO2 52,74 51,7 52,23 52,1 Al2O3 1,4 1,37 1,7 - ZrO2 3,39 3,38 3,0 3,0 ZnO 7,83 5,48 7,6 7,6 CuO - - - 1,8 SrO 7,12 6,98 6,4 6,4 BaO 14,75 18,9 14,9 14,9 Li2O 1,23 1,21 1,5 1,5 Na2O 5,96 5,84 5,7 5,7 K2O 7,38 7,28 7,3 7,3 TiO2 - - 0,81 0,81 CeO2 - - 0,66 0,66 Sb2O3 0,39 0,4 0,4 0,4
  2. Gläser nach Anspruch 1,
    dadurch gekennzeichnet, daß
    sie weitgehend aus den folgenden Zusammensetzungen bestehen, ausgedrückt in Gewichtsprozent auf Oxidbasis, SiO2 53-62 ZnO 8-13 Li2O 0-2 SrO+BaO+ZnO 27-32 Na2O 2-7 CaO 0-5 K2O 3-11 Al2O3 0-3 Li2O+Na2O+K2O 8-14 ZrO2 0-4 SrO 0-3 SiO2+Al2O3+ZrO2 56-65 BaO 15-19
  3. Gläser nach Anspruch 1 oder 2, weiterhin enthaltend bis zu insgesamt 0,1 % mindestens eines Übergangsmetalloxids oder eines Seltenerdmetalloxids.
  4. Tischgeschirr und/oder Zierkristallglaswaren, bestehend aus Gläsern die weitgehend frei von Blei sind,
    dadurch gekennzeichnet, daß
    sie eine Dichte von mindestens 2,9 g/cm3 und einen Brechungsindex von mindestens 1,545 aufweisen und weitgehend aus den folgenden Zusammensetzungen bestehen, ausgedrückt in Gewichtsprozent auf Oxidbasis, SiO2 51-63 Al2O3 0-5 Li2O 0-3 ZrO2 0-6 Na2O 0-8 SiO2+Al2O3+ZrO2 55-66 K2O 0-12 TiO2 0-3 Li2O+Na2O+K2O 7-15 CaO 0-5 SrO 0-<8 MgO 0-3 BaO >13-21 B2O3 0-3 ZnO 5-15 La2O3 0-8 SrO+BaO+ZnO 27-34
  5. Tischgeschirr und/oder Zierkristallglaswaren nach Anspruch 4,
    dadurch gekennzeichnet, daß
    sie weitgehend aus den folgenden Zusammensetzungen bestehen, ausgedrückt in Gewichtsprozent auf Oxidbasis, SiO2 53-62 ZnO 8-13 Li2O 0-2 SrO+BaO+ZnO 27-32 Na2O 2-7 CaO 0-5 K2O 3-11 Al2O3 0-3 Li2O+Na2O+K2O 8-14 ZrO2 0-4 SrO 0-3 SiO2+Al2O3+ZrO2 56-65 BaO 15-19
  6. Tischgeschirr und/oder Zierkristallglaswaren nach Anspruch 4 oder 5, weiterhin enthaltend bis zu insgesamt 0,1 % mindestens eines Übergangsmetalloxids oder Seltenerdmetalloxids.
EP94118661A 1993-12-10 1994-11-28 Bleifreie Gläser mit Kristalleigenschaften Expired - Lifetime EP0657391B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9314881 1993-12-10
FR9314881A FR2713622B1 (fr) 1993-12-10 1993-12-10 Verres ne contenant pas de plomb et présentant les caractéristiques du cristal.

Publications (2)

Publication Number Publication Date
EP0657391A1 EP0657391A1 (de) 1995-06-14
EP0657391B1 true EP0657391B1 (de) 2000-05-03

Family

ID=9453815

Family Applications (1)

Application Number Title Priority Date Filing Date
EP94118661A Expired - Lifetime EP0657391B1 (de) 1993-12-10 1994-11-28 Bleifreie Gläser mit Kristalleigenschaften

Country Status (9)

Country Link
US (1) US5468693A (de)
EP (1) EP0657391B1 (de)
JP (1) JPH07257936A (de)
BR (1) BR9404896A (de)
CA (1) CA2137122C (de)
DE (1) DE69424263T2 (de)
ES (1) ES2145804T3 (de)
FR (1) FR2713622B1 (de)
RU (1) RU2129100C1 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2614756C1 (ru) * 2016-03-15 2017-03-29 Юлия Алексеевна Щепочкина Глазурь

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JP2906104B2 (ja) * 1992-10-20 1999-06-14 東洋ガラス 株式会社 鉛を含まないクリスタルなガラス組成物
IT1268814B1 (it) * 1994-12-13 1997-03-06 Calp Spa Miscela vetrificabile per vetri di qualita'
JP3666054B2 (ja) * 1995-04-14 2005-06-29 日本電気硝子株式会社 基板用ガラス
TW402579B (en) * 1996-06-07 2000-08-21 Toyo Glass K K Production method for lead- free crystal glass composition
KR100238117B1 (ko) * 1996-12-05 2000-01-15 박영구 프라즈마 영상표시판넬용 기판유리조성물
DE19650692C2 (de) * 1996-12-06 1999-01-14 Schott Glas Bleifreie Krongläser
WO1998040491A2 (en) * 1997-03-13 1998-09-17 Mycogen Corporation Pesticidal bacillus thuringiensis strains
JP2002522346A (ja) * 1998-08-14 2002-07-23 コーニング インコーポレイテッド 鉛を含まないガラス
DE19936699C2 (de) * 1999-08-04 2001-10-31 Nachtmann F X Bleikristall Blei- und bariumfreies Kristallglas
JP2001139341A (ja) 1999-11-11 2001-05-22 Nippon Sheet Glass Co Ltd 屈折率分布型レンズ用母材ガラス組成物
FR2826955B1 (fr) * 2001-07-09 2003-10-03 Snc Eurokera Verre mineral sans plomb, email obtenu avec celui-ci
JP2005170720A (ja) * 2003-12-10 2005-06-30 Asahi Glass Co Ltd 陰極線管パネルガラス
JP2006188406A (ja) * 2005-01-07 2006-07-20 Asahi Glass Co Ltd 平板ディスプレイ用真空外囲器およびそれを用いた平板ディスプレイ
CN111533444A (zh) * 2020-05-14 2020-08-14 承德华富玻璃技术工程有限公司 一种无铅水晶器皿及其制备工艺
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Publication number Priority date Publication date Assignee Title
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Also Published As

Publication number Publication date
JPH07257936A (ja) 1995-10-09
BR9404896A (pt) 1995-08-08
RU94044493A (ru) 1996-10-27
CA2137122C (en) 2004-06-15
DE69424263T2 (de) 2000-10-19
ES2145804T3 (es) 2000-07-16
RU2129100C1 (ru) 1999-04-20
US5468693A (en) 1995-11-21
EP0657391A1 (de) 1995-06-14
CA2137122A1 (en) 1995-06-11
FR2713622A1 (fr) 1995-06-16
DE69424263D1 (de) 2000-06-08
FR2713622B1 (fr) 1996-03-01

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